Alumina/Silicon Carbide Laminated Composites by Spark Plasma Sintering

Ceramic laminates composed of alumina/silicon carbide composite layers were produced by spark plasma sintering (SPS). Monolithic composite disks containing up to 30 vol% of silicon carbide were fabricated by stacking together and cosintering by SPS green layers prepared by tape casting water-based suspensions. An engineered laminate with a specific layer combination that is able to promote the stable growth of surface defects before final failure was also designed and produced. Fully dense materials with an optimum adhesion between the constituting layers and a homogeneous distribution of the two phases were obtained after SPS. Monolithic composites showed an increasing strength with SiC load, and biaxial strength values as high as 700 MPa were observed for a SiC content of 30 vol%. The engineered laminate showed a peculiar crack propagation that is responsible for the high strength value of about 600 MPa and for the evident insensitivity to surface defects.     

Silicon Carbide/Calcium Aluminosilicate: A Notch-Insensitive Ceramic-Matrix Composite

Tension experiments performed on a 0/90 laminated silicon carbide/calcium aluminosilicate composite at room temperature establish that this material is notch insensitive. Multiple matrix cracking is determined to be the stress redistribution mechanism. This mechanism is found to provide a particularly efficient means for creating local inelastic strains, which eliminate stress concentrations.     

Tensile Creep and Creep-Strain Recovery Behavior of Silicon Carbide Fiber/Calcium Aluminosilicate Matrix Ceramic Composites

The tensile creep and creep strain recovery behavior of 0° and 0°/90° Nicalon-fiber/calcium aluminosilicate matrix composites was investigated at 1200°C in high-purity argon. For the 0° composite, the 100-h creep rate ranged from approximately 4.6 × 10⁻⁹ s⁻¹ at 60 MPa to 2.2 × 10⁻⁸ s⁻¹ at 200 MPa. At 60 MPa, the creep rate of the 0°/90° composite was approximately the same as that found for the 0° composite, even though the 0°/90° composite had only one-half the number of fibers in the loading direction. Upon unloading, the composites exhibited viscous strain recovery. For a loading history involving 100 h of creep at 60 MPa, followed by 100 h of recovery at 2 MPa, approximately 27% of the prior creep strain was recovered for the 0° composite and 49% for the 0°/90° composite. At low stresses (60 and 120 MPa), cavities formed in the matrix, but there was no significant fiber or matrix damage. For moderate stresses (200 MPa), periodic fiber rupture occurred. At high stresses (250 MPa), matrix fracture and rupture of the highly stressed bridging fibers limited the creep life to under 70 min.     

Creep Anisotropy of a Continuous-Fiber-Reinforced Silicon Carbide/Calcium Aluminosilicate Composite

Creep studies conducted on a unidirectional silicon carbide calcium aluminosilicate composite indicate that the Nicalon fibers provide longitudinal creep strengthening at 1200°C. The deformation is transient in nature because grain growth in the fibers enhances their creep resistance. The' transverse creep strength is considerably smaller, being dominated by the matrix, resulting in appreciable creep anisotropy. This anisotropy leads to severe distortion when off-axis loadings are imposed. Residual stresses develop upon unloading alter creep, and cause superficial matrix cracking.     

Silicon Carbide Platelet/Silicon Carbide Composites

α-silicon carbide platelet/β-silicon carbide composites have been produced in which the individual platelets were coated with an aluminum oxide layer. Hot-pressed composites showed a fracture toughness as high as 7.2 MPa·m^1/2. The experiments indicated that the significant increase in fracture toughness is mainly the result of crack deflection and accompanying platelet pullout. The coating on the platelets also served to prevent the platelets from acting as nucleation sites for the α- to β-phase transformation, so that the advantageous microstructure remains preserved during high-temperature processing.     

Silicon Carbide/Silicon and Silicon Carbide/Silicon Carbide Composites Produced by Chemical Vapor Infiltration

Composites of SiC/Si and SiC/SiC were prepared from single yarns of SiC. The use of carbon coatings on SiC yarn prevented the degradation normally observed when chemically vapor deposited Si is applied to SiC yarn. The strength, however, was not retained when the composite was heated at elevated temperatures in air. In contrast, the strength of a SiC/C/SiC composite was not reduced after this composite was heated at elevated temperatures, even when the fiber ends were exposed.     

Effect of Quasi-Static Loading Rate on Damage Formation in Silicon Carbide Reinforced Calcium Aluminosilicate Unidirectional Composites

For experiments at higher and lower loading rates, significant differences in the mechanical responses of unidirectional silicon carbide reinforced calcium aluminosilicate composites were observed. Axial and transverse stress–strain measurements, acoustic emission measurements, and post-test microstructural observations all indicated that there are changes in the sequence and extent of the formation of damage. The differences are attributed to rate-dependent matrix cracking due to environmental effects and rate dependencies associated with the fiber–matrix interface.     

Mechanical Properties of Alumina/Silicon Carbide Whisker Composites

The improvement of mechanical properties of Al₂O₃/SiC whisker composites has been studied with emphasis on the effects of the whisker content and of the hot-pressing temperature. Mechanical properties such as fracture toughness and fracture strength increased with increasing whisker content up to 40 wt%. In the case of the high SiC whisker content of 40 wt%, fracture toughness of the sample hot-pressed at 1900° decreased significantly, in spite of densification, compared with one hot-pressed at 1850°. Fracture toughness strongly depended on the microstructure, especially the distribution of SiC whiskers rather than the grain size of the Al₂O₃ matrix.     

Thermomechanical Fatigue Behavior of a Silicon Carbide Fiber-Reinforced Calcium Aluminosilicate Composite

Isothermal fatigue and in-phase thermomechanical fatigue (TMF) tests were performed on a unidirectional, continuous-fiber, Nicalon®-reinforced calcium aluminosilicate glass-ceramic composite ([O]_16, SiC/CAS-II). Monotonic tensile tests were performed at 1100°C (2012°F) and 100 MPa/s (14.5 ksi/s) to determine the material's ultimate strength (σ_ult) and proportional limit (σ_pl). Isothermal fatigue tests at 1100°C employed two loading profiles, a triangular waveform with ramp times of 60 s and a similar profile with a superimposed 60-s hold time at σ_max. All fatigue tests used a σ_max of 100 MPa (40% of σ_pl), R = 0.1. TMF loading profiles were identical to the isothermal loading profiles, but the temperature was cycled between 500° and 1100°C (932° and 2012°F). All fatigued specimens reached run-out (1000 cycles) and were tested in tension at 1100°C immediately following the fatigue tests. Residual modulus, residual strength, cyclic stress-strain modulus, and strain accumulation were all examined as possible damage indicators. Strain accumulation allowed for the greatest distinction to be made among the types of tests performed. Fiber and matrix stress analyses and creep data for this material suggest that matrix creep is the primary source of damage for the fatigue loading histories investigated.     

Elastic Properties and Microcracking Behavior of Particulate Titanium Diboride–Silicon Carbide Composites

The spontaneous microcracking of particulate TiB₂–SiC composites is studied as a function of TiB₂ volume fraction. The degree of microcracking was examined by measuring elastic properties from room temperature to 1300°C. The results showed that only one composition contains microcracks. All other compositions did not microcrack regardless of TiB₂ volume fraction. This was attributed to the difference in the sintering aids. In particular, the Al₂O₃ sintering aid needed in these compositions had reacted with SiO₂ to form an amorphous grain boundary phase that allowed residual stresses to relax by viscous flow at moderate to high temperatures. The existence of this amorphous grain boundary phase was directly observed by transmission electron microscopy.     

Experimental Observations of High Fracture Resistance in Silicon Carbide/Alumina Laminated Composites

Model laminated composites were fabricated with porous-Al₂O₃ interfaces between SiC bars. The porous Al₂O₃ was deposited using an aerosol spray deposition technique, and the sandwich specimen was fabricated by hot pressing. Residual thermal stresses were present in the interface because of the difference in the coefficients of thermal expansion of SiC and Al₂O₃. Crack deflection was observed with measured interfacial fracture resistances that were considerably higher than the deflection threshold predicted by the He–Hutchinson criterion. Examination of the fracture surface revealed a tortuous crack path and significant crack–flaw interaction.     

Stress-Corrosion Cracking of Silicon Carbide Fiber/Silicon Carbide Composites

Ceramic-matrix composites are being developed to operate at elevated temperatures and in oxidizing environments. Considerable improvements have been made in the creep resistance of SiC fibers and, hence, in the high-temperature properties of SiC fiber/SiC (SiC_f/SiC) composites; however, more must be known about the stability of these materials in oxidizing environments before they are widely accepted. Experimental weight change and crack growth data support the conclusion that the oxygen-enhanced crack growth of SiC_f/SiC occurs by more than one mechanism, depending on the experimental conditions. These data suggest an oxidation embrittlement mechanism (OEM) at temperatures <1373 K and high oxygen pressures and an interphase removal mechanism (IRM) at temperatures of ≳700 K and low oxygen pressures. The OEM results from the reaction of oxygen with SiC to form a glass layer on the fiber or within the fiber–matrix interphase region. The fracture stress of the fiber is decreased if this layer is thicker than a critical value ( d > d _c) and the temperature below a critical value ( T < T _g), such that a sharp crack can be sustained in the layer. The IRM results from the oxidation of the interfacial layer and the resulting decrease of stress that is carried by the bridging fibers. Interphase removal contributes to subcritical crack growth by decreasing the fiber-bridging stresses and, hence, increasing the crack-tip stress. The IRM occurs over a wide range of temperatures for d < d _c and may occur at T > T _g for d > d _c. This paper summarizes the evidence for the existence of these two mechanisms and attempts to define the conditions for their operation.     

Microstructure, Phase and Thermoelastic Properties of Laminated Liquid-Phase-Sintered Silicon Carbide–Titanium Carbide Ceramic Composites

Hot-pressed silicon carbide–titanium carbide (SiC—TiC) composites sintered with liquid-phase forming Al₂O₃ and Y₂O₃ mixtures have been studied. Samples were fabricated by successively stacking tape-cast sheets of a single composition, resulting in a laminated body of uniform composition. This approach required the development of a technology easily transferable into the production of functionally graded SiC–TiC materials. The effects of this processing route on the resultant microstructures and phases were explored in detail. Additionally, because of the consequences for graded materials, the effects of TiC proportion on the thermal expansion coefficients, Young's modulus, and Poisson's ratios for several SiC–TiC composites were also determined.     

Reaction Bonding and Mechanical Properties of Mullite/Silicon Carbide Composites

Based on the RBAO technology, low-shrinkage mullite/SiC/ Al₂O₃/ZrO₂ composites were fabricated. A powder mixture of 40 vol% Al, 30 vol% A1₂O₃ and 30 vol% SiC was attrition milled in acetone with TZP balls which introduced a substantial ZrO₂ wear debris into the mixture. The precursor powder was isopressed at 300–900 MPa and heattreated in air by two different cycles resulting in various phase ratios in the final products. During heating, Al oxidizes to Al₂O₃ completely, while SiC oxidizes to SiO₂ only on its surface. Fast densification (at >1300°C) and mullite formation (at 1400°C) prevent further oxidation of the SiC particles. Because of the volume expansion associated with the oxidation of Al (28%), SiC (108%), and the mullitization (4.2%), sintering shrinkage is effectively compensated. The reaction-bonded composites exhibit low linear shrinkages and high strengths: shrinkages of 7.2%, 4.8%, and 3%, and strengths of 610, 580, and 490 MPa, corresponding to compaction pressure of 300, 600, and 900 MPa, respectively, were achieved in samples containing 49–55 vol% mullite. HIPing improved significantly the mechanical properties: a fracture strength of 490 MPa and a toughness of 4.1 MPa^.m^1/2 increased to 890 MPa and 6 MPa^.m^1/2, respectively.     

Silicon Carbide Platelet/Alumina Composites: II, Mechanical Properties

The mechanical properties, i.e., Young's modulus, fracture toughness, and flexural strength, of SiC-platelet/Al₂O₃ composites with two different platelet sizes were studied. Both Young's modulus and the fracture toughness of composites using small platelets (12 μm) increased with increasing SiC volume fraction. Maximum values for toughness and Young's modulus of 7.1 MPa·m^1/2 and 421 GPa were obtained for composites containing 30 vol% platelets. Composites fabricated using larger platelets (24 μm), however, showed spontaneous microcracking at SiC volume fractions of ≤0.15. The presence of microcracks decreased Young's modulus and the fracture toughness substantially. Two types of radial microcracks were identified by optical microscopy and found to be consistent with a residual stress analysis. Anisotropy in fracture toughness was identified with a crack length indentation technique. Cracks propagating in a plane parallel to platelet faces experienced the least resistance, which was the the lowest toughness plane in platelet composites with preferred orientation. Enhanced fracture toughness was found in the plane parallel to the hot-pressing direction, but no anisotropy in toughness was observed in this plane. The flexural strength of alumina showed a decrease from 610 to 480 MPa for a 30 vol% composite and was attributed to the presence of the platelets.     

Elastic Properties and Structure of Interpenetrating Boron Carbide/Aluminum Multiphase Composites

We study the elastic moduli and structure of boron carbide/aluminum (B₄C/Al) multiphase composites using rigorous bounding and experimental characterization techniques. We demonstrate that rigorous bounds on the effective moduli are useful in that they can accurately predict (i) the effective elastic moduli, given the phase moduli and volume fractions, or (ii) the phase moduli (volume fractions), given the effective moduli and phase volume fractions (moduli). Using the best available rigorous bounds on the effective elastic moduli of multiphase composites involving volume-fraction information, we are able to predict the bulk and shear moduli of the Al₄BC phase, a reaction product that forms during heat treatment. These theoretical predictions are in very good agreement with recent experimental measurements of the moduli of the Al₄BC phase. Moreover, we evaluate more-refined bounds involving three-point structural correlation functions by extracting such information from an image of a sample of the B₄C/Al composite. Although experimental data for the effective moduli are unavailable for this sample, our predictions of the effective moduli based on three-point bounds should be quite accurate.     

Effect of Composition on Properties of Alumina/Titanium Silicon Carbide Composites

In the present study, the room-temperature properties of Al₂O₃-Ti₃SiC₂ composites with different Ti₃SiC₂ contents are determined. The composites are prepared by attrition milling Al₂O₃ and Ti₃SiC₂ mixture powders followed by spark plasma sintering (SPS) under vacuum. From a closer examination of the dependencies of the electrical conductivity on compositions in this system, we determined the percolation threshold at which an interconnected network of electrically conductive phase arises. Since the hardness of Ti₃SiC₂ is lower than that of Al₂O₃, the Vickers hardness decreased with the increasing of Ti₃SiC₂ content while the fracture toughness and the strength increased. The maximum strength (673 MPa) and the maximum toughness (9.3 MPa·m^1/2) were reached in the pure Ti₃SiC₂ material.     

Microstructure of Silicon Carbide/Carbon Composites and Relationships with Mechanical Properties

Three different 2-D SiC/C composites, analyzed by TEM, have mechanical performances directly controlled by the interfacial structure resulting from processing. Localized attachment of the fibers to a brittle matrix constituent is shown to be responsible for composite weakening by impeding interface debonding and sliding. Moreover, the particulate phase used in the matrix is found to have a strong influence. There is a consequent sensitivity of composite strength to the particulate properties. Finally, it is demonstrated that the hindrance of debonding and sliding caused by the brittle matrix phase can be suppressed by using a C fiber coating.     

Thermal Expansion of Laminated, Woven, Continuous Ceramic Fiber/Chemical-Vapor-Infiltrated Silicon Carbide Matrix Composites

Thermal expansions of three two-dimensional laminate, continuous fiber/chemical-vapor-infiltrated silicon carbide matrix composites reinforced with either FP-Alumina (alumina), Nextel (mullite), or Nicalon (Si-C-O-N) fibers are reported. Experimental thermal expansion coefficients parallel to a primary fiber orientation were comparable to values calculated by the conventional rule-of-mixtures formula, except for the alumina fiber composite. Hysteriesis effects were also observed during repeated thermal cycling of that composite. Those features were attributed to reoccurring fiber/matrix separation related to the micromechanical stresses generated during temperature changes and caused by the large thermal expansion mismatch between the alumina fibers and the silicon carbide matrix.